Log in

View Full Version : RDX and elements for procedure - Archive File


megalomania
June 21st, 2003, 11:23 AM
Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 04-10-2001 03:57 PM
--------------------------------------------------------------------------------
I have a few questions about the procedure for making RDX from hexamine:
1) to make the hexamine, does it have to be 36% formaldehyde mixed with 30% ammonia water or can it be like 40%formaldehyde with 25% ammonia?

2) when stabilizing the RDX with ammonium nitrate, to make composition Amex, what has to be done, should the mixing be done while wet? What is a practical way to stabilize RDX?

3) My procedure says that when all the hexamine is added, to bring the temp to 0 degrees and keep there for twenty minutes. I have read conflicting info, could someone tell me something about this?

4) 550ml of red nitric acid with 50g hexamine seems like a fuckload, can I use less and still obtain a decent yeild or are there methods of acid recovery?

Your input will be much appreciated!



FadeToBlackened
Frequent Poster
Posts: 201
From: Hell
Registered: MAR 2001
posted 04-10-2001 04:59 PM
--------------------------------------------------------------------------------
Well in response to question 1:
Yes, but you'd have to adjust your reactants accordingly. e.g.: using quite a bit more ammonia..
dont ask me how much though hehe



Jumala
Frequent Poster
Posts: 202
From: Germany
Registered: OCT 2000
posted 04-10-2001 06:59 PM
--------------------------------------------------------------------------------
-- OOOH MY GOD --
Look here

http://huizen.dds.nl/~arcticus/synthesis.htm

or here

http://internettrash.com/users/megalomania/explosives.html




Igenx
Frequent Poster
Posts: 80
From: No Fucking Way
Registered: SEP 2000
posted 04-10-2001 11:56 PM
--------------------------------------------------------------------------------
Hmm. That was an intresting read. Guess I'll have to look at that again when I dream about producing RDX.


Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 04-22-2001 02:54 PM
--------------------------------------------------------------------------------
Well, I have opted to take the paraformaldehyde, ammonium nitrate, acetic anhydride route to making RDX. I figger you waste a lot less chemicals, and it is more simple. I am using Mega's recipe. I think for the yield it should be 30g should the reaction go well. Though, there are two parts in this recipe which i am concerned about. This is when you raise the temp to 90c after mixing the AN with the acetic anhydride. COULD THIS BLOW ME UP??? (I don't think so, but still a little concerned since in this field all you need is a tiny mistake and you're a crispy, chunky, critter!) Also, when I am adding the paraformaldehyde, there are no specifications in Mega's recipe as for JUST HOW SLOWLY TO ADD IT.
Any knowledge you can share would be much appreciated.



Mr Cool
Frequent Poster
Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 04-23-2001 01:13 PM
--------------------------------------------------------------------------------
If you don't know how slowly, do it very slowly to be safe.
Where are you getting you acetic anhydride?


Detonator
Frequent Poster
Posts: 133
From:
Registered: NOV 2000
posted 04-24-2001 02:07 AM
--------------------------------------------------------------------------------
Temp should not be above 90c you better watch out cause you would never control the reaction.
Add paraformaline as 3-5grams and wait untill the reaction stops.
Always keep cold water next to you...if the temp was going up fast you have to put what ever your using in the cold water untill you see the reaction is getting quit, then take it out of it.




Demolition
Frequent Poster
Posts: 158
From: Australia
Registered: FEB 2001
posted 04-24-2001 03:22 AM
--------------------------------------------------------------------------------
Detonator,when you say
quote:
--------------------------------------------------------------------------------
put what ever your using in the cold water untill you see the reaction is getting quit, then take it out of it.
--------------------------------------------------------------------------------

Do you mean pour the contents of what your making into the cold water or do you mean to put the container what your using into the cold water so it will take out the heat out of the reaction?
Demolition
-------------------------------
The Ultimate Machine......XR650
-------------------------------



PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 04-24-2001 08:30 AM
--------------------------------------------------------------------------------
I would say put it in water and run away..don't look at it...runaway reaction can be much faster than you to put it in cold water and cool down..any nitroglycerin experienced guy could tell you this...a little heat and suddenly boiling, red fumes,..fire or explosion if further in the process..hot acid is not something you want on you skin!
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"



Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 04-27-2001 04:29 AM
--------------------------------------------------------------------------------
Thanks people. Paraformaline = paraformaldehyde right, duh, sorry. Paraformaldehyde can be obtained by boiling down 40% formaldehyde to get a solid and then drying that out, right? Well, acetic anhydride is no problem over here in Kenya, I have access to tons of it!!!! Any chemical company sells it to me or I just go to schools and get it from the labs. About the reaction, how long should I wait after heating the ammonium nitrate/acetic anhydride mix to 90c, to what temp should it cool down before adding paraformaldehyde? Should I put in ice bath? cool bath or something?


Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 05-01-2001 03:51 PM
--------------------------------------------------------------------------------
Maybe the following should be in a reply to one of the nitric acid topics, but this is "...and elements for procedure" meaning any procedure, ie, W, K, E processes. SO, I took some nitric acid and attempted to concentrate it by placing two erlehnmeyer flasks joined by glass piping and closed with rubber stoppers, one of the flasks contained about 20ml of 70% nitric and the other contained about 100ml of nitric and was placed in a very cold ice bath. To the first a formaldehyde(37%) drip was attached. NO2 bubbled to the other one and the experiment was concluded in about 1hr. What turned out in the second beaker was a mixture of rubber and NO2 fuming nitric acid. that was pretty stupid so I guess I could distill it (without vacuum) and reobtain unpoluted nitric? Also I tried the experiment again, this time without rubber stoppers, and my product was orange nitric acid that fumed NO2 dark red fumes. HOW DO I KNOW IF THIS IS 95%-100% concentration? Any comments on my procedure or product or answers to my questions would be great.


Cyware
New Member
Posts: 22
From: Nomatter
Registered: APR 2001
posted 05-01-2001 07:08 PM
--------------------------------------------------------------------------------
Paraformaldehyde can't be obtained by boiling a solution of formaldehyde (I tried and all I obtained was nothing than a STRONG stink of formaldehyde in my house). The industrial method involves the vaporization of formaldehyde solution at vacuum, because if you heat it the formaldehyde will vaporise faster than the water.
With vacuum method the result will be like (CHO)n, where n=25-50, so a polimer with maximum 50 molecules of formaldehyde. That's why you have to procure the paraformaldehyde. Sadly, the polimerisation reaction can't be started with sulfuric acid, like for acetaldehyde upper aldehydes.
I have an old bottle of formaldehyde and I plan to use the paraformaldehyde wich is on the bottom of the bottle for RDX synthesis. I still have no more then 10 grams, but this should be enough for 20 g of RDX.


PHILOU Zrealone
Frequent Poster
Posts: 479
From: Brussels,Belgium,Europe
Registered: SEP 2000
posted 05-03-2001 09:05 AM
--------------------------------------------------------------------------------
Upon standing 40% formaline lead to a white precipitate of paraformaldehyde (C3H6O3) and polyformal((-CH2-O)n!
I have a 1L old bottle (4 years) of formaline 40% and nearly 1/5 of it is a solid white paste of those products!
------------------
"Life that deadly disease sexually transmitted".
"Chemistry is all what stinks and explode; Physic is all what never works! ;-p :-) :o)"



Cyware
New Member
Posts: 22
From: Nomatter
Registered: APR 2001
posted 05-03-2001 07:07 PM
--------------------------------------------------------------------------------
Hmmm... I didn't know that paraformaldehyde is the trimeric form of formaline. I thought that paraformaldehyde is the polimeric form. So, no RDX synthesis Saturday (as I planned)...


fightclub
New Member
Posts: 39
From: none
Registered: APR 2001
posted 05-03-2001 08:11 PM
--------------------------------------------------------------------------------
Paraformaldehyde (which has been falsely called trioxymethylene) has the composition: HO.CH2.O.[CH2.O]x.CH2.OH. Paraformaldehyde is a mixture of polymer-homologous Polyoxymethylene glycols, which probably contain 10-50 H2C=O molecules.


Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 05-11-2001 02:31 AM
--------------------------------------------------------------------------------
Paraformaldehyde has proven to be very difficult to obtain...I made summor nitric acid and it is a DARK GREEN color, could this be contaminated? It fumes like a fucker. Or is it that color at high concentrations? How do I know when it is almost pure?





Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 06-04-2001 04:20 PM
--------------------------------------------------------------------------------
OK, pretty good, now I have my RDX. Should I bother mixing it with other compounds to stabilize it or something? I have set it to air dry, and made fucking sure before that it was neutral to litmus and purified it by dissolving in acetone and then recrystalizing. SO, what now, will it react with metals or some weird shit like that? Does it matter too much what kinda container I detonate it in?


Mr Cool
Frequent Poster
Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 06-05-2001 05:43 AM
--------------------------------------------------------------------------------
I seem to remember hearing that HNO2, not HNO3, was green, so maybe you have this instead.
Conc. HNO3 definately isn't green.


Mr Cool
Frequent Poster
Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 06-05-2001 04:03 PM
--------------------------------------------------------------------------------
RDX is safe with everything I know of that you might mix it with. Al and Cu tubes are OK for detonators.


Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 06-05-2001 05:29 PM
--------------------------------------------------------------------------------
Ok, the RDX is dry. I am going to run some drop tests to see how sensitive it is. Does anyone have info on drop tests for RDX? First I will try a 1kg weight from 10cm. If this is two sensitive then I will mix it with some potassium nitrate, I heard this is a way to desensitize it. My source says "small amount" of potassium nitrate is needed to desensitize the RDX. I wish these sources were not so fucking vague sometimes. How the hell much is a small amount? Should the mixing be done while RDX is wet?
------------------




HNIW
Frequent Poster
Posts: 46
From: Poland
Registered: JAN 2001
posted 06-06-2001 04:01 AM
--------------------------------------------------------------------------------
For RDX you have to drop 2kg from 30-32 cm. In comparison for tetryl you need 2kg from 40cm.
Sources:
"Chemistry and technology of explosives" T. Urbański


Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 06-09-2001 05:51 PM
--------------------------------------------------------------------------------
Got a beautiful RDX detonation, blew up an abandoned shack of dimensions of about 400ft squared. Got it on film, shit flew everywhere.
Thanx for the info people. By the way, why does the nitric acid used in the production of RDX have to be free of NOx fumes? since I did not use a process that required nitric acid I did not have to free my nitric acid of these fumes. I hear adding urea to it frees it of NOx fumes, what ratio is used in addition? How much urea to how much nitric?

Ps HNIW have you ever made HNIW? not wishing to divert from the topic of this post but anyways just curious.



Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 06-09-2001 05:55 PM
--------------------------------------------------------------------------------
Sorry, Hit reply button to early.
I determined that the RDX was stable enough to use alone. But how much Potassium nitrate would be needed to desensitize it?



simply RED
Frequent Poster
Posts: 242
From: HELL
Registered: OCT 2000
posted 06-10-2001 03:50 AM
--------------------------------------------------------------------------------
Dhzugasvili, what was the exact process that you used to produce the RDX, the one with paraformaldehyde, AN and Acetic anhydride?
Where did you find the anhydride from?


Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 06-10-2001 04:52 AM
--------------------------------------------------------------------------------
Simply Red, read my answer above for where I obtained acetic anhydride, over here we don't have law problems.




Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 06-12-2001 04:07 PM
--------------------------------------------------------------------------------
Well, Looks like my project to make RDX has been completed, but I am still left with these major questions for which I seek answers:
1)How much Potassium Nitrate is needed to stabilize RDX and when in the procedure is this added to the RDX crystals? While still wet? Is this a reliable way of stabilizing it without loosing detonation velocity?

2) To make RDX using a process which utilizes nitric acid, does the nitric have to be free of NO2 fumes? Are the fumes eliminated by adding urea to it (nitric)? How much is added to how much nitric, or until it becomes clear and no more fumes are seen?

3) this might be a stupid question, but how can one tell whether the acid is really 96%+ above concentration? If the acid appears green, then it is possibly that it has a high percentage of HNO2

4) and finally, how long can RDX last in storage? psst!... I still have some!

Please, oh pretty PleAsE, AnsWeR My QuEstIOns, or I will die or something...



simply RED
Frequent Poster
Posts: 242
From: HELL
Registered: OCT 2000
posted 06-12-2001 04:37 PM
--------------------------------------------------------------------------------
I see!
You are lucky to find chemicals easy. Here I must fight with chem supliers for every bottle of chemical(last time they wanted my phone). Bulgaria is not a nice plasce for pyros like me.
1. You need very little KNO3(few percents) to stabilize the RDX. Add the very fine powdered KNO3 to the very fine powdered RDX. It will be stabilized, but you may left your RDX clear. It won't change for years if ever.
2. Use pure nitric acid 99+ to make RDX. Add very little urea(crystaline or saturated solution). Less than a percent.
3. The conc. nitric acid must be red because of free NO2. It should become colorless after the urea has been added.
4. RDX can be stored forever.


Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 06-14-2001 06:20 PM
--------------------------------------------------------------------------------
Spaciba (thank you) Simply Red! My mind is like the arrow of Confuscious's thought. It's path can be fully straightened with the answer to one last question:
I have read conflicting info that red fuming nitric acid has to be used for the K process or the simple hexamine nitration process, and that white acid (urea added) must be used. Which one of these two statements is bullshit?



simply RED
Frequent Poster
Posts: 242
From: HELL
Registered: OCT 2000
posted 06-15-2001 04:03 PM
--------------------------------------------------------------------------------
Priwet Toware6!
It is said that the acid must be free of NO2. So, concentrated acid with very little urea must be used. Someone claim that acid with little NO2 also works.
I have tried the process with not 99% HNO3, it was white and the yield was awful if it was pure RDX.


Mr Cool
Frequent Poster
Posts: 1013
From: None of your bloody business!
Registered: DEC 2000
posted 06-16-2001 09:37 AM
--------------------------------------------------------------------------------
The amount of urea needed depends on the NO2 concentration. About 2% works for the acid that I distill.
If you don't use strong enough acid (more than about 95% I believe), you'll get lots of hexamine dinitrate, which will mostly dissolve, making it appear that you got a shitty yield of RDX, when all you have is hexamine dinitrate!
Use the method with 99% white HNO3 and anhydrous ammonium nitrate. This reacts with the formaldehyde produced to make more RDX, thus greatly improving the yields!
Just curious: Can 100% HNO3 be stored for extended periods of time? I thought it might decompose too fast, and that is why you can normally get a maximum of about 80% from chemical suppliers. I've never tried to store it, but it'd be more convenient for me to make a large batch and keep it until I need it.



Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 06-17-2001 05:10 PM
--------------------------------------------------------------------------------
still on the subject of nitric acid, Mr. Cool said that
"I seem to remember hearing that HNO2, not HNO3, was green, so maybe you have this instead.
Conc. HNO3 definately isn't green"
If indeed it is HNO2 that I have, can in be converted into HNO3 by cooling to 5degrees celcius and bubbling O2 through it? I have read this somewhere I am sure, but not sure about the validity of the information. If so, how do ya generate the O2? By the way, I have posted a topic on this in MISCELLANEOUS.



Dhzugasvili
Frequent Poster
Posts: 64
From:
Registered: APR 2001
posted 07-26-2001 06:12 PM
--------------------------------------------------------------------------------
my last reply to this topic is old and not a query anymore so ignore, but now I am interested in making RDX via the following process:
75g hexamine is dissolved in 120ml pure nitric acid keeping temp between 20 to 30 deg C. once all hex dissolved soln heated to 55degC for 10 min and then diluted with 750ml and then purified the usual way with acetone.

How reliable/efficient is this process??



Hex
Frequent Poster
Posts: 82
From: Glasgow, Scotland, UK
Registered: JUL 2001
posted 07-30-2001 01:29 PM
--------------------------------------------------------------------------------
tioxymethylene exists (i used it today!) and is the cyclic trimer of formaldehyde, as opposed to a polymer. It's useful for reactions in solvents where paraform is insoluble.